Effect of carrier size on the dispersion of salmeterol xinafoate from interactive mixtures

The objective of this study was to determine the influence of lactose carrier size on drug dispersion of salmeterol xinafoate (SX) from interactive mixtures. SX dispersion was measured by using the fine particle fractions determined by a twin stage impinger attached to a Rotahaler1. The particle size of the lactose carrier in the SX interactive mixtures was varied using a range of commercial inhalation-grade lactoses. In addition, differing size fractions of individual lactose samples were achieved by dry sieving. The dispersion ofSXappeared to increase as the particle size of the lactose carrier decreased for the mixtures prepared from different particle size commercial samples of lactose and from different sieve fractions of the same lactose. Fine particles of lactose (<5 mm) associated with the lactose carrier were removed from the carrier surface by a wet decantation process to produce lactose samples with low but similar concentrations of fine lactose particles. The fine particle fractions of SX in mixtures prepared with the decanted lactose decreased significantly (analysis of variance, p<0.001) and the degree of dispersion became independent of the volume mean diameter of the carriers (analysis of variance, p<0.05). The dispersion behavior is therefore associated with the presence of fine adhered particles associated with the carriers and the inherent size of the carrier itself has little influence on dispersion.

Lactose surface modification by decantation: Are drug-fine lactose ratios the key to better dispersion of salmeterol xinafoate from lactose-interactive mixtures?

Purpose The role of fine lactose in the dispersion of salmeterol xinafoate (SX) from lactose mixtures was studied by modifying the fine lactose concentration on the surface of the lactose carriers using wet decantation. Methods Fine lactose was removed from lactose carriers by wet decantation using ethanol saturated with lactose. Particle sizing was achieved by laser diffraction. Fine particle fractions (FPFs) were determined by Twin Stage Impinger using a 2.5% SX mixture, and SX was analyzed by a validated high-performance liquid chromatography method. Adhesion forces between probes of SX and silica and the lactose surfaces were determined by atomic force microscopy. Results FPFs of SX were related to fine lactose concentration in the mixture for inhalation grade lactose samples. Reductions in FPF (2-4-fold) of Aeroflo 95 and 65 were observed after removing fine lactose by wet decantation; FPFs reverted to original values after addition of micronized lactose to decanted mixtures. FPFs of SX of sieved and decanted fractions of Aeroflo carriers were significantly different (p < 0.001). The relationship between FPF and fine lactose concentration was linear. Decanted lactose demonstrated surface modification through increased SX-lactose adhesion forces; however, any surface modification other than removal of fine lactose only slightly influenced FPF. Conclusions Fine lactose played a key and dominating role in controlling FPF. SX to fine lactose ratios influenced dispersion of SX with maximum dispersion occurring as the ratio approached unity.

Criteria for interpreting kimberlite as coherent: Insights from the Muskox and Jericho kimberlites (Nunavut, Canada)

The Jurassic Muskox and Jericho kimberlites (Northern Slave Province, Nunavut, Canada) contain a variety of facies exhibiting different geometries, contact relationships, internal organisation, country rock abundance and olivine shapes, although many have similar matrix/groundmass mineralogies and textures. Five facies are examined that either have characteristics consistent with coherent rocks in general (i.e. intrusive and extrusive non-fragmental rocks) or are mineralogically and texturally similar to kimberlite described as coherent (or apparent coherent). Three facies are interpreted as coherent on the basis of: (1) geological setting, (2) apparent-porphyritic texture, (3) sharp contacts with fragmental kimberlite, (4) relative abundance of elongate and unbroken olivine crystals and (5) paucity of country rock xenoliths, while the remaining two facies are interpreted as fragmental on the basis of: (1) the gradational contacts with demonstrably fragmental kimberlite, (2) relative abundance and range of sizes of country rock lithic clasts and (3) numerous broken olivine crystals. Comparisons are made with coherent and apparent-coherent kimberlite from the literature. Our three coherent facies are similar to literature reported coherent kimberlite dykes hosted in country rock (CKd) in terms of internal organisation, low abundance of country rock xenoliths, and apparent-porphyritic texture. Conversely, our two fragmental facies share attributes with previously described pipe-filling coherent and apparent-coherent kimberlite (CKpf) in terms of geometry, internal organisation and abundance of country rock xenoliths. We conclude that CKd and most CKpf, although similar in matrix/groundmass mineralogy and texture, can be distinguished on the basis of internal organisation, country rock lithic clast abundance, texture (e.g. apparent-porphyritic texture) and possibly olivine crystal shapes and suggest that fragmental kimberlite is more common than reported.

A comprehensive mechanistic kinetic model for dilute acid hydrolysis of switchgrass cellulose to glucose, 5-HMF and levulinic acid

Switchgrass was treated by 1% (w/w) H₂SO₄in batch tube reactors at temperatures ranging from 140–220°C for up to 60 minutes. In this study, release patterns of glucose, 5-hydroxymethylfurfural (5-HMF), and levulinic acid from switchgrass cellulose were investigated through a mechanistic kinetic model. The predictions were consistent with the measured products of interest when new parameters reflecting the effects of reaction limitations, such as cellulose crystallinity, acid soluble lignin–glucose complex (ASL–glucose) and humins that cannot be quantitatively analyzed, were included. The new mechanistic kinetic model incorporating these parameters simulated the experimental data with R² above 0.97. Results showed that glucose yield was most sensitive to variations in the parameter regarding the cellulose crystallinity at low temperatures (140–180°C), while the impact of crystallinity on the glucose yield became imperceptible at elevated temperatures (200–220 °C). Parameters related to the undesired products (e.g. ASL–glucose and humins) were the most sensitive factors compared with rate constants and other additional parameters in impacting the levulinic acid yield at elevated temperatures (200–220°C), while their impacts were negligible at 140–180°C. These new findings provide a more rational explanation for the kinetic changes in dilute acid pretreatment performance and suggest that the influences of cellulose crystallinity and undesired products including ASL–glucose and humins play key roles in determining the generation of glucose, 5-HMF and levulinic acid from biomass-derived cellulose.

An efficient hole transport material composite based on poly(3-hexylthiophene) and bamboo-structured carbon nanotubes for high performance perovskite solar cells

In this work, we have developed a new efficient hole transport material (HTM) composite based on poly(3- hexylthiophene) (P3HT) and bamboo-structured carbon nanotubes (BCNs) for CH3NH3PbI3 (MAPbI3) based perovskite solar cells. Compared to pristine P3HT, it is found that the crystallinity of P3HT was significantly improved by addition of BCNs, which led to over one order of magnitude higher conductivity for the composite containing 1–2 wt% BCNs in P3HT. In the meantime, the interfacial charge transfer between the MAPbI3 light absorbing layer and the HTM composite layer based on P3HT/BCNs was two-fold faster than pristine P3HT. More importantly, the HTM film with a superior morphological structure consisting of closely compact large grains was achieved with the composite containing 1 wt% BCNs in P3HT. The study by electrochemical impedance spectroscopy has confirmed that the electron recombination in the solar cells was reduced nearly ten-fold with the addition of 1 wt% carbon nanotubes in the HTM composite. Owing to the superior HTM film morphology and the significantly reduced charge recombination, the energy conversion efficiency of the perovskite solar cells increased from 3.6% for pristine P3HT to 8.3% for P3HT/(1 wt% BCNs) with a significantly enhanced open circuit voltage (Voc) and fill factor (FF). The findings of this work are important for development of new HTM for high performance perovskite solar cells.

Calcium phosphate flocs and the clarification of sugar cane juice from whole of crop harvesting

Sugar cane biomass is one of the most viable feedstocks for the production of renewable fuels and chemicals. Therefore, processing the whole of crop (WC) (i.e., stalk and trash, instead of stalk only) will increase the amount of available biomass for this purpose. However, effective clarification of juice expressed from WC for raw sugar manufacture is a major challenge because of the amounts and types of non-sucrose impurities (e.g., polysaccharides, inorganics, proteins, etc.) present. Calcium phosphate flocs are important during sugar cane juice clarification because they are responsible for the removal of impurities. Therefore, to gain a better understanding of the role of calcium phosphate flocs during the juice clarification process,the effects of impurities on the physicochemical properties of calcium phosphate flocs were examined using small-angle laser light scattering technique, attenuated total reflectance Fourier transformed infrared spectroscopy, and X-ray powder diffraction. Results on synthetic sugar juice solutions showed that the presence of SiO2 and Na+ ions affected floc size and floc structure. Starch and phosphate ions did not affect the floc structure; however, the former reduced the floc size, whereas the latter increased the floc size. The study revealed that high levels of Na+ ions would negatively affect the clarification process the most, as they would reduce the amount of suspended particles trapped by the flocs. A complementary study on prepared WC juice using cold and cold/intermediate liming techniques was conducted. The study demonstrated that, in comparison to the one-stage (i.e., conventional) clarification process, a two-stage clarification process using cold liming removed more polysaccharides (≤19%),proteins (≤82%), phosphorus (≤53%), and SiO2 (≤23%) in WC juice but increased Ca2+ (≤136%) and sulfur (≤200%)

Pre-lithiation of onion-like carbon/MoS2 nano-urchin anodes for high-performance rechargeable lithium ion batteries

Hybrid urchin-like nanostructures composed of a spherical onion-like carbon (OLC) core and MoS2 nanoleaves were synthesized by a simple solvothermal method followed by thermal annealing treatment. Compared to commercial MoS2 powder, MoS2/OLC nanocomposites exhibit enhanced electrochemical performance as anode materials of lithium-ion batteries (LIBs) with a specific capacity of 853 mA h g−1 at a current density of 50 mA g−1 after 60 cycles, and a moderate initial coulombic efficiency of 71.1%. Furthermore, a simple pre-lithiation method based on direct contact of lithium foil with MoS2/OLC nano-urchins was used to achieve a very high coulombic efficiency of 97.6% in the first discharge/charge cycle, which is at least 26% higher compared to that of pristine MoS2/OLC nano-urchins. This pre-lithiation method can be generalized to develop other carbon-metal sulfide nanohybrids for LIB anode materials. These results may open up a new avenue for the development of the next-generation high-performance LIBs.

Evaluation of CaO-CeO2-partially stabilized zirconia thermal barrier coatings

Plasma sprayable powders were prepared from ZrO2-CaO-CeO2 system using an organic binder and coated onto stainless steel substrates previously coated by a bond coat (Ni 22Cr 20Al 1.0Y) using plasma spraying. The coatings exhibited good thermal barrier characteristics and excellent resistance to thermal shock at 1000 degrees C under simulated laboratory conditions (90 half hour cycles without failure) and at 1200 degrees C under accelerated burner rig test conditions (500 2 min cycles without failure). No destabilization of cubic/tetragonal ZrO2 phase fraction occured either during the long hours (45 h cumulative) or the large number of thermal shock tests. Growth of a distinct SiO2 rich region within the ceramic was observed in the specimens thermal shock cycled at 1000 degrees C apart from mild oxidation of the bond coat. The specimens tested at 1200 degrees C had a glassy appearance on the top surface and exhibited severe oxidation of the bond coat at the ceramic-bond coat interface. The glassy appearance of the surface is due to the formation of a liquid silicate layer attributable to the impurity phase present in commercial grade ZrO2 powder. These observations are supported by SEM analysis and quantitative EDAX data.

Structure of KNb0.5OPO4, a KTiOPO4 analog

The crystal structure of KNb0.5V0.5OPO4, a new KTiOPO4 isomorph, has been refined from powder X-ray diffraction data by Rietveld refinement. The structure is orthorhombic, space group Pna2(1), with a = 12.933(1), b = 6.4713(8), and c = 10.7273(6) Angstrom, Z = 8. There is a preferential distribution of Nb(V) and V(III) atoms in the octahedral M(1) [0.806Nb, 0.194V] and M(2) [0.194Nb, 0.806V] sites, the M(1)O-6 octahedra being more distorted than the M(2)O-6 octahedra. The results are compared with other KTiOPO4 derivatives.

Increasing ionic conductivity and mechanical strength of a plastic electrolyte by inclusion of a polymer

in this contribution we present a soft matter solid electrolyte which was obtained by inclusion of a polymer (polyacrylonitrile, PAN) in LiClO4/LiTFSI-succinonitrile (SN), a semi-solid organic plastic electrolyte. Addition of the polymer resulted in considerable enhancement in ionic conductivity as well as mechanical strength of LiX-SN (X=ClO4, TFSI) plastic electrolyte. Ionic conductivity of 92.5%-[1 M LiClO4-SN]:7.5%-PAN (PAN amount as per SN weight) composite at 25 degrees C recorded a remarkably high value of 7 x 10(-3) Omega(-1) cm(-1), higher by few tens of order in magnitude compared to 1 M LiClO4-SN. Composite conductivity at sub-ambient temperature is also quite high. At -20 degrees C, the ionic conductivity of (100 -x)%-[1 M LiClO4-SN]:x%-PAN composites are in the range 3 x 10(-5)-4.5 x 10(-4) Omega(-1) cm(-1), approximately one to two orders of magnitude higher with respect to 1 M LiClO4-SN electrolyte conductivity. Addition of PAN resulted in an increase of the Young's modulus (Y) from Y -> 0 for LiClO4-SN to a maximum of 0.4MPa for the composites. Microstructural studies based on X-ray diffraction, differential scanning calorimetry and Fourier transform infrared spectroscopy suggest that enhancement in composite ionic conductivity is a combined effect of decrease in crystallinity and enhanced trans conformer concentration. (c) 2008 Elsevier Ltd. All rights reserved.

Determination of refractive and volatile elements in sediment using laser ablation inductively coupled plasma mass spectrometry

Wet-milling protocol was employed to produce pressed powder tablets with excellent cohesion and homogeneity suitable for laser ablation (LA) analysis of volatile and refractive elements in sediment. The influence of sample preparation on analytical performance was also investigated, including sample homogeneity, accuracy and limit of detection. Milling in volatile solvent for 40 min ensured sample is well mixed and could reasonably recover both volatile (Hg) and refractive (Zr) elements. With the exception of Cr (−52%) and Nb (+26%) major, minor and trace elements in STSD-1 and MESS-3 could be analysed within ±20% of the certified values. Comparison of the method with total digestion method using HF was tested by analysing 10 different sediment samples. The laser method recovers significantly higher amounts of analytes such as Ag, Cd, Sn and Sn than the total digestion method making it a more robust method for elements across the periodic table. LA-ICP-MS also eliminates the interferences from chemical reagents as well as the health and safety risks associated with digestion processes. Therefore, it can be considered as an enhanced method for the analysis of heterogeneous matrices such as river sediments.

Synthesis, structure and properties elf a new ternary interstitial nitride: Ni2W3N

A new ternary interstitial nitride Ni2W3N has been synthesized by the ammonolysis of different oxide precursors and characterized by powder X-ray diffraction and electron microscopy. This nitride crystallizes in the cubic space group P4(1)32(213) [Ni2W3N, a=6.663(1) Angstrom, Z=4] and is isostructural with Al2Mo3C. This compound belongs to the rare class of intermetallic ternary nitrides and carbides crystallizing with a filled beta-Mn structure. Ni2W3N is not stable, it decomposes to a new compound NiW3N related to the distorted anti-perovskite, Ca3AsN structure.

Fabrication and evaluation of 1 Ah silver/metal hydride cells

Silver/metal hydride (Ag/MH) cells of about 1 Ah capacity have been fabricated and their discharge characteristics at different rates of discharge, faradaic efficiency, cycle life and a.c. impedance have been evaluated. These cells comprise metal-hydride electrodes prepared by employing similar to 60 mu m powder of an AB(2)-Laves phase alloy of nominal composition Zr0.5Ti0.5V0.6Cr0.2Ni1.2 with PTFE binder on a nickel-mesh substrate as the negative plates and commercial-grade silver electrodes as the positive plates. The cells are positive limited and exhibit two distinct voltage plateaus characteristic of two-step reduction of AgO to Ag during their low rates of discharge between C/20 and C/10. This feature is, however, absent when the cells are discharged at C/5 rate. On charging the cells to 100% of their capacity, the faradaic efficiency is found to be 100%. The impedance of the Ag/MH cell is essentially due to the impedance of the silver electrodes, since MH electrodes offer negligible impedance. The cells may be subjected to a large number of charge-discharge cycles with little deterioration.

Phase transitions and rare-earth magnetism in hexagonal and orthorhombic $DyMnO_{3}$ single crystals

The floating-zone method with different growth ambiences has been used to selectively obtain hexagonal or orthorhombic DyMnO3 single crystals. The crystals were characterized by x-ray powder diffraction of ground specimens and a structure refinement as well as electron diffraction. We report magnetic susceptibility, magnetization and specific heat studies of this multiferroic compound in both the hexagonal and the orthorhombic structure. The hexagonal DyMnO3 shows magnetic ordering of Mn3+ (S = 2) spins on a triangular Mn lattice at T-N(Mn) = 57 K characterized by a cusp in the specific heat. This transition is not apparent in the magnetic susceptibility due to the frustration on the Mn triangular lattice and the dominating paramagnetic susceptibility of the Dy3+ (S = 9/2) spins. At T-N(Dy) = 3 K, a partial antiferromagnetic order of Dy moments has been observed. In comparison, the magnetic data for orthorhombic DyMnO3 display three transitions. The data broadly agree with results from earlier neutron diffraction experiments, which allows for the following assignment: a transition from an incommensurate antiferromagnetic ordering of Mn3+ spins at T-N(Mn) = 39 K, a lock-in transition at Tlock-in = 16 K and a second antiferromagnetic transition at T-N(Dy) = 5 K due to the ordering of Dy moments. Both the hexagonal and the orthorhombic crystals show magnetic anisotropy and complex magnetic properties due to 4f-4f and 4f-3d couplings.

Phase Equilibria in the System $Al_{2}O_{3}-CaO-CoO$ and Gibbs Energy of Formation of $Ca_{3}CoAl_{4}O_{10}$

The floating-zone method with different growth ambiences has been used to selectively obtain hexagonal or orthorhombic DyMnO3 single crystals. The crystals were characterized by x-ray powder diffraction of ground specimens and a structure refinement as well as electron diffraction. We report magnetic susceptibility, magnetization and specific heat studies of this multiferroic compound in both the hexagonal and the orthorhombic structure. The hexagonal DyMnO3 shows magnetic ordering of Mn3+ (S = 2) spins on a triangular Mn lattice at T-N(Mn) = 57 K characterized by a cusp in the specific heat. This transition is not apparent in the magnetic susceptibility due to the frustration on the Mn triangular lattice and the dominating paramagnetic susceptibility of the Dy3+ (S = 9/2) spins. At T-N(Dy) = 3 K, a partial antiferromagnetic order of Dy moments has been observed. In comparison, the magnetic data for orthorhombic DyMnO3 display three transitions. The data broadly agree with results from earlier neutron diffraction experiments, which allows for the following assignment: a transition from an incommensurate antiferromagnetic ordering of Mn3+ spins at T-N(Mn) = 39 K, a lock-in transition at Tlock-in = 16 K and a second antiferromagnetic transition at T-N(Dy) = 5 K due to the ordering of Dy moments. Both the hexagonal and the orthorhombic crystals show magnetic anisotropy and complex magnetic properties due to 4f-4f and 4f-3d couplings.